تفاعل #76776

ord-f44e1b90f39141189916bd77ce99a78d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe solution was heated at 80° to 90° C. for 40 minutes
  2. 2
    أخرىobtained
  3. 3
    workup.ADDITIONabove was added
  4. 4
    ترشيحThe precipitated crystals were collected by filtration
  5. 5
    أخرىdried under reduced pressure, which

الإجراء التجريبي

Then, 49.2 g of sodium acetate and 40.5 g of 1,1-dibromo-3,3,3-trifluoroacetone were dissolved in 400 ml of water, and the solution was heated at 80° to 90° C. for 40 minutes. The solution was cooled to 0° C., to which 75 g of the crude 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride crystals obtained above was added, and the mixture was stirred at room temperature for 70 minutes. The precipitated crystals were collected by filtration and dried under reduced pressure, which afforded 35.4 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-hydroxyphenylhydrazone).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06703503B2uspto-grants-2004_03